Polymer ( IF 4.1 ) Pub Date : 2022-08-31 , DOI: 10.1016/j.polymer.2022.125268 Monika Flejszar , Kinga Ślusarczyk , Paweł Chmielarz , Joanna Smenda , Karol Wolski , Magdalena Wytrwal-Sarna , Marcin Oszajca
Facile, low-cost, and environmentally friendly procedures for the synthesis of hybrid materials are highly desirable for industrial applications and large-scale synthesis. To meet these needs, this paper presents an ultra-simple, organic solvent-free and yet effective method for the synthesis of hybrid materials consisting of an inorganic core and an organic layer of poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA) brushes. Bearing in mind the numerous works published in recent years on the synthesis of PDMAEMA via “normal” and low ppm ATRP using additional reductants or complicated and expensive apparatus, e.g. a photoreactor or potentiostat, this article is a step forward, reducing the costs of the process and increasing the safety of the experimenter. In order to develop the title “facile recipe” a series of reactions aimed at optimizing the synthesis conditions in which the monomer plays a dual role and participates simultaneously as a reducing agent according to the activators regenerated by electron transfer (ARGET) atom transfer radical polymerizations (ATRP) were carried out. As a result, an in-depth analysis of the synthesis conditions and the influence of the presence of oxygen allowed the development of a monomer-mediated ATRP procedure inspired by the principles of green chemistry. Finally, 30 ppm of CuIIBr2/TPMA (where TPMA: tris(2-pyridylmethyl)amine) and 20 μl/cm2 of the reaction mixture were used to obtain a homogeneous polymeric brush layer with the thickness of 331 nm, which was revealed by atomic force microscopy (AFM) measurements. Additionally, the presence and composition of the obtained polymer brushes were confirmed by X-ray photoelectron spectroscopy (XPS) analyses and scanning electron microscope (SEM) with imaging of elemental composition on the decorated silicon surface.
中文翻译:
实验室工作台上的 SI-ATRP:使用微升体积的试剂合成耐氧 PDMAEMA 刷子的简便配方
用于合成杂化材料的简便、低成本和环境友好的程序对于工业应用和大规模合成是非常理想的。为了满足这些需求,本文提出了一种超简单、无有机溶剂且有效的方法,用于合成由无机核和聚(2-(二甲基氨基)甲基丙烯酸乙酯有机层)(PDMAEMA)组成的杂化材料。刷子。铭记近年来发表的大量关于 PDMAEMA 合成的著作“正常”和低 ppm ATRP 使用额外的还原剂或复杂而昂贵的设备,例如光反应器或恒电位仪,这篇文章是向前迈出的一步,降低了过程的成本并提高了实验者的安全性。为了开发名为“简易配方”的一系列反应,旨在优化合成条件,其中单体发挥双重作用并根据电子转移(ARGET)原子转移自由基聚合再生的活化剂同时作为还原剂参与(ATRP)进行。结果,对合成条件和氧气存在的影响的深入分析允许开发受绿色化学原理启发的单体介导的 ATRP 程序。最后,30 ppm 的 Cu II Br2 /TPMA(其中TPMA:三(2-吡啶基甲基)胺)和20μl/cm 2的反应混合物用于获得厚度为331nm的均匀聚合物刷层,通过原子力显微镜(AFM)显示) 测量。此外,通过 X 射线光电子能谱 (XPS) 分析和扫描电子显微镜 (SEM) 确认了所获得的聚合物刷的存在和组成,并对装饰硅表面上的元素组成进行了成像。